CN108287171A - The detection method of battery electrode paste dispersed homogeneous degree and application - Google Patents
The detection method of battery electrode paste dispersed homogeneous degree and application Download PDFInfo
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- CN108287171A CN108287171A CN201711499196.3A CN201711499196A CN108287171A CN 108287171 A CN108287171 A CN 108287171A CN 201711499196 A CN201711499196 A CN 201711499196A CN 108287171 A CN108287171 A CN 108287171A
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Abstract
The invention discloses a kind of detection method of battery electrode paste dispersed homogeneous degree and application, the detection method includes：The Black-White of standard sample pole piece made from the normal electrode slurry by known dispersed homogeneous degree is measured, standard parameter range is obtained；The Black-White of the pole piece to be measured made of electrode slurry to be measured is measured, detected value is obtained；It is on the contrary then do not meet if the detected value within the scope of the standard parameter, judges that the dispersed homogeneous degree of the electrode slurry to be measured meets the requirements.The present invention detects the pole piece brightness (Black-White) after slurry drying using Black-White meter, non-destructive indirectly judges slurry dispersed homogeneous degree and provides concrete numerical value, reduce the raw material needed for examining, it effectively increases the yield of product, production efficiency, reduce cost of labor, can be applied to the detection of large-scale production.
Description
Technical field
The present invention is more particularly directed to a kind of detection method of battery electrode paste dispersed homogeneous degree and applications.
Background technology
Pulp of lithium ion battery mixing dispersing technology is in the entire production technology of lithium ion battery to the quality shadow of product
Loudness is more than 30%, is most important link in entire production technology, but at present in the production process of lithium ion battery, battery
Consistency control is still the technological difficulties that lithium ion battery makes, in addition, being constantly progressive with lithium ion battery material, former
Material granule grain size is smaller and smaller, and which not only improves performance of lithium ion batteries, is also easily created two level aggregate, to
Increase the difficulty of mixing dispersing technology.In lithium ion battery production process, it should focus on to pay close attention to the mixing dispersion of positive and negative electrode slurry
Uniform situation.
The be uniformly dispersed mode of situation of the mixing of existing detection slurry generally has：Detect apparent viscosity, the difference of slurry
Density, solid content and the granularity etc. that dispersion is examined using Hegman grind gage of layer, existing detection mode generally need to be sampled repeatedly,
Raw material are wasted, are taken longer and larger by environmental error, instrument error, human error；Although being come using SEM Electronic Speculum straight
Slurry deployment conditions are observed although connecing directly effectively, cost is too big and time-consuming longer, also higher for the attainment requirement of employee,
Large-scale production should not be extended to.
Invention content
The main purpose of the present invention is to provide a kind of detection method of battery electrode paste dispersed homogeneous degree and application, with
Overcome the deficiencies in the prior art
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes：
An embodiment of the present invention provides a kind of detection methods of battery electrode paste dispersed homogeneous degree, including：
The Black-White of standard sample pole piece made from the normal electrode slurry by known dispersed homogeneous degree is measured, standard is obtained
Parameter area；
The Black-White of the pole piece to be measured made of electrode slurry to be measured is measured, detected value is obtained；
If the detected value within the scope of the standard parameter, judges the dispersed homogeneous degree symbol of the electrode slurry to be measured
It closes and requires, it is on the contrary then do not meet.
The embodiment of the present invention additionally provides a kind of production method of lithium ion battery, including：
Using the dispersed homogeneous degree of the detection method detection lithium ion battery anode glue size or negative electrode slurry；And
If it is determined that the dispersed homogeneous degree of the lithium ion battery anode glue size or negative electrode slurry is qualified, then lithium-ion electric is carried out
The preparation of pond positive or negative pole, conversely, then re-starting decentralized processing to the lithium ion battery anode glue size or negative electrode slurry.
Compared with prior art, advantages of the present invention includes：After the present invention detects slurry drying using Black-White meter
Pole piece brightness (Black-White), non-destructive indirectly judge slurry dispersed homogeneous degree and provide concrete numerical value, reduce inspection institute
The raw material needed effectively increases the yield of product, production efficiency, reduces cost of labor, can be applied to the inspection of large-scale production
It surveys.
Description of the drawings
Fig. 1 a are the electron microscopes that positive LiFePO4 slurry amplifies 1000 times in an exemplary embodiments of the invention；
Fig. 1 b are the electron microscopes that positive LiFePO4 slurry amplifies 5000 times in an exemplary embodiments of the invention；
Fig. 1 c are the electron microscopes that positive LiFePO4 slurry amplifies 10000 times in an exemplary embodiments of the invention；
Fig. 2 a are the electron microscopes that cathode electrographite slurry amplifies 500 times in an exemplary embodiments of the invention；
Fig. 2 b are the electron microscopes that cathode electrographite slurry amplifies 1000 times in an exemplary embodiments of the invention；
Fig. 2 c are the electron microscopes that cathode electrographite slurry amplifies 3000 times in an exemplary embodiments of the invention；
Fig. 3 is positive plate Black-White test position schematic diagram in an exemplary embodiments of the invention；
Fig. 4 is negative plate Black-White test position schematic diagram in an exemplary embodiments of the invention；
Fig. 5 is the overhaul flow chart of battery electrode paste dispersed homogeneous degree in an exemplary embodiments of the invention.
Specific implementation mode
In view of deficiency in the prior art, inventor is able to propose the present invention's through studying for a long period of time and largely putting into practice
Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.
An embodiment of the present invention provides a kind of detection methods of battery electrode paste dispersed homogeneous degree, including：
The Black-White of standard sample pole piece made from the normal electrode slurry by known dispersed homogeneous degree is measured, standard is obtained
Parameter area；
The Black-White of the pole piece to be measured made of electrode slurry to be measured is measured, detected value is obtained；
If the detected value within the scope of the standard parameter, judges the dispersed homogeneous degree symbol of the electrode slurry to be measured
It closes and requires, it is on the contrary then do not meet.
Preferably, the dispersed homogeneous degree of the normal electrode slurry is found out by SEM Electronic Speculum observed patterns.
In some more specific embodiment, the detection method includes：In such a way that colour difference meter directly measures
Obtain the Black-White of standard sample pole piece and pole piece to be measured.
Preferably, the colour difference meter includes Black-White meter.
In some more specific embodiment, the detection method includes：It measures on the standard sample pole piece
The Black-White of more than two difference inspection positions, to obtain the standard parameter range.
In some more specific embodiment, the detection method includes：Two are measured on the pole piece to be measured
The Black-White of the above difference inspection positions later detects the two or more to obtain more than two detected values
Value is compared with the standard parameter range.
Further, all components and each component content all same of the normal electrode slurry and electrode slurry to be measured.
In some more specific embodiment, the detection method includes：By electrode slurry to be measured in vacuum ring
Pole piece to be measured is formed after being dried under border.
Further, the battery electrode paste includes lithium ion battery anode glue size or negative electrode slurry.
The embodiment of the present invention additionally provides a kind of production method of lithium ion battery, including：
Using the dispersed homogeneous degree of the detection method detection lithium ion battery anode glue size or negative electrode slurry；And
If it is determined that the dispersed homogeneous degree of the lithium ion battery anode glue size or negative electrode slurry is qualified, then lithium-ion electric is carried out
The preparation of pond positive or negative pole, conversely, then re-starting decentralized processing to the lithium ion battery anode glue size or negative electrode slurry.
In some more specific embodiment, the dispersion of anode or negative electrode slurry mixing is observed by SEM Electronic Speculum
Uniformity, then by colour difference meter carry out Black-White detection obtain its corresponding numberical range, as the later stage judgement foundation；
A certain amount of anode or negative electrode slurry are taken in mixed processes, base material is uniformly coated onto using four sides film applicator
On, be placed in vacuum drying oven, after drying, the detection of Black-White carried out using colour difference meter, by the obtained Black-White of detection again with
Critical field is compared, and then judges that slurry has been uniformly dispersed in critical field.
In painting process, then the detection of Black-White can be carried out using colour difference meter directly by positive plate or negative plate, it will
It detects obtained Black-White to be compared with critical field again, raw material in the coat on base material is then judged in critical field
It is to be uniformly dispersed.
1. experiment accumulation data obtain the critical field stage：
Electrode slurry is obtained by the material mixture ratio in table 1：
1 electrode slurry of table matches
Electrode slurry is prepared according to the proportioning in table 1, and at least obtains above-mentioned electrode slurry in such a way that SEM Electronic Speculum is observed
The situation that is uniformly dispersed (3. 1. electrographite slurry illustrates for LiFePO4 slurry and cathode using anode), determines above-mentioned electrode
After slurry is uniformly dispersed, numerical value on the basis of being counted as first using calibration plate white tile calibration Black-White；Reuse four sides film applicator
Finely dispersed slurry is coated on base material, drying in vacuum drying oven is placed on and obtains pole piece, and place vacuum tank
Interior room temperature preservation is cooled to room temperature；Finally Black-White meter is used to carry out the detection of Black-White to pole piece, obtains following Black-White model
It encloses as shown in table 2：
Table 2 is the Black-White range of the pole piece made from the electrode slurry in table 1
Black-White is ranging from according to the Black-White range of pole piece made from the electrode slurry in table 1 in table 2, to change electricity
The each component ratio of pole slurry then needs to test obtaining Black-White range again.
2. the application stage
2.1 mixed processes
According to the slurry that production SOP is completed, few slurry sample is taken.Calibration plate white tile calibration Black-White meter is used first
As numerical benchmark；It reuses four sides film applicator finely dispersed slurry is coated on base material, is placed on vacuum drying oven
Interior drying, and place room temperature preservation in vacuum tank and be cooled to room temperature；Black-White meter is finally used to carry out pole piece obtained black
The detection of whiteness.And be compared with critical field, production slurry is transferred to subsequent processing if in range；If not meeting
In range, then extend mixing jitter time and dispersion linear velocity until reaching in critical field.
Embodiment 1
Slurry mixing is carried out according to following proportioning：LiFePO4 94wt%, conductive agent 2wt%, Kynoar 4wt%.
(1) liquid NMP is transferred in blending tank body by liquid automatical feeding system, solid content is set according to 45wt%
Count (i.e. LiFePO4+conductive agent+Kynoar=100wt%, powder ratio, slurry ratio-powder：Liquid NMP=
55wt%：45wt%)
(2) by powder automatical feeding system by powder Kynoar, control is added in 30min to mixing tank body
Interior, adition process need to open dispersion and revolution；
(3) after the completion of Kynoar is added, dispersion and revolution linear velocity is improved, 1.5h is stirred；
(4) powder conductive agent is added by powder automatical feeding system, and controls and adds to mixing tank body in 10min
Interior, adition process need to open dispersion and revolution；
(5) after the completion of conductive agent is added, dispersion and revolution linear velocity is improved, 1.5h is stirred；
(6) by powder automatical feeding system by the LiFePO4 of 50% mass of powder, control is added in 10min to mixed
It closes in tank body, adition process need to open dispersion and revolution；
After the completion of the LiFePO4 of (7) 50% mass enters, dispersion and revolution linear velocity are improved, 1h is stirred；
(8) LiFePO4 of remaining 50% mass of powder is added in 10min by control by powder automatical feeding system
It adds to blending tank body, adition process need to open dispersion and revolution；
(9) after the completion of the LiFePO4 of residue 50wt% enters, dispersion and revolution linear velocity is improved, 1h is stirred；
(10) dispersion is closed, revolution and vacuumize process slurry are only opened, stirs 1h：
(11) 50ml beakers are used to sample vacuumize process slurry；
(12) by the base material for sampling the platform that slurry is poured on four sides film, adjustment scraper starts film to 80-120 μm；
(13) base material of film is placed in vacuum drying oven, vacuum drying oven has been heated to 90 DEG C at this time, and the time sets
Set 5min；Film on base material has dried the NMP liquid eliminated in slurry, and is adhesive into pole piece with base material, takes out
Pole piece is cooled to room temperature, and is controlled in 10min；
(14) it opens Black-White meter pole piece cooling time, preheats and use calibration plate white tile calibration as base value
Value；
(15) pole piece is stably placed in detection platform (marble top), starts to measure Black-White numerical value, it is right
The different location of same pole piece is detected (see Fig. 3 and Fig. 4), and obtains the gray value at different location：76,78,81,84,
In the range of 81 ± 8；
Embodiment 2
Slurry mixing is carried out according to following proportioning：Electrographite 97wt%, conductive agent 0.5wt%, CMC1wt%,
SBR1.5wt%；
(1) liquid D W deionized waters are transferred in blending tank body by liquid automatical feeding system, solid content according to
50wt% is designed；
(2) by powder automatical feeding system by powder CMC, control is added to blending tank body in 30min, was added
Journey need to open dispersion and revolution；
(3) after the completion of CMC is added, dispersion and revolution linear velocity is improved, 1.5h is stirred；
(4) control is added in powder conductive agent by powder automatical feeding system to add to blending tank body in 10min,
Adition process need to open dispersion and revolution；
(5) after the completion of conductive agent is added, dispersion and revolution linear velocity is improved, 1.5h is stirred；
(6) electrographite of powder 50wt% mass is added control and added in 10min by powder automatical feeding system
It is complete in blending tank body, adition process need to open dispersion and revolution；
After the completion of the electrographite of (7) 50% mass enters, dispersion and revolution linear velocity are improved, 1h is stirred；
(8) electrographite of remaining 50% mass of powder is added in 10min by control by powder automatical feeding system
It adds to blending tank body, adition process need to open dispersion and revolution；
(9) after the completion of the electrographite of remaining 50% mass enters, dispersion and revolution linear velocity is improved, 1h is stirred；
(10) SBR and vacuumize process slurry is added, stirs 1h；
(11) 50ml beakers are used to sample vacuumize process slurry；
(12) by the base material for sampling the platform that slurry is poured on four sides film, adjustment scraper starts film to 80-120 μm；
(13) base material of film is placed in vacuum drying oven, vacuum drying oven has been heated to 90 DEG C at this time, and the time sets
Set 5min；Film on base material has dried the DW liquid eliminated in slurry, and is adhesive into pole piece with base material.Take out pole
Piece is cooled to room temperature, and is controlled in 10min.
(14) it opens Black-White meter pole piece cooling time, preheats and use calibration plate white tile calibration as base value
Value.
(15) pole piece is stably placed on platform (marble top), starts to measure Black-White numerical value, to same
The different location of pole piece is detected this numerical value (see figure)：62；60；66；66, in the range of 62 ± 10.
Painting process：
According to the slurry that production SOP is completed, and painting process is completed, Black-White meter uses calibration plate white board school first
Standard is used as numerical benchmark；Pole piece is placed from coating winding extraction is steady in Black-White meter detection platform；Finally use Black-White
Meter carries out the detection of Black-White to it.And contrast standard range, if production slurry is transferred to subsequent processing in range；If no
Meet in range, then extends mixing jitter time and dispersion linear velocity until reaching in critical field.
Embodiment 3
Slurry mixing is carried out according to following proportioning：LiFePO4 94wt%, conductive agent 2wt%, Kynoar 4wt%；
Specific steps obtain pole piece with reference to embodiment 1 and embodiment 2, and pole piece is stably placed on platform (marble
Desktop), start to measure Black-White numerical value, this numerical value (see figure) is detected to the different location of same pole piece：77；
78；83；86, in the range of 81 ± 8.
Compared with prior art, the present invention detects the pole piece brightness (Black-White) after slurry drying using Black-White meter,
Non-destructive indirectly judges slurry dispersed homogeneous degree and provides concrete numerical value, reduces the raw material needed for examining, effectively improves
The yield of product, reduces cost of labor at production efficiency, can be applied to the detection of large-scale production.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
According to equivalent change or modification made by spirit of the invention, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of detection method of battery electrode paste dispersed homogeneous degree, it is characterised in that including：
The Black-White of standard sample pole piece made from the normal electrode slurry by known dispersed homogeneous degree is measured, standard parameter is obtained
Range；
The Black-White of the pole piece to be measured made of electrode slurry to be measured is measured, detected value is obtained；
If the detected value within the scope of the standard parameter, judges that the dispersed homogeneous degree of the electrode slurry to be measured conforms to
It asks, it is on the contrary then do not meet.
2. detection method according to claim 1, it is characterised in that：The dispersed homogeneous degree of the normal electrode slurry is logical
Cross what SEM Electronic Speculum observed patterns were found out.
3. detection method according to claim 1, it is characterised in that including：It is marked in such a way that colour difference meter directly measures
The Black-White of quasi- sample pole piece and pole piece to be measured.
4. detection method according to claim 3, it is characterised in that：The colour difference meter includes Black-White meter.
5. detection method according to any one of claim 1-3, it is characterised in that including：Measure the standard sample grade
The Black-White of the more than two different inspection positions of on piece, to obtain the standard parameter range.
6. detection method according to claim 1, it is characterised in that including：Measure on the pole piece to be measured it is more than two not
With the Black-White of inspection positions, to obtain more than two detected values, later by more than two detected values and institute
Standard parameter range is stated to be compared.
7. detection method according to claim 1, it is characterised in that：The normal electrode slurry and electrode slurry to be measured
All components and each component content all same.
8. detection method according to claim 1, it is characterised in that including：Electrode slurry to be measured is dried under vacuum environment
Pole piece to be measured is formed after dry.
9. detection method according to claim 1, it is characterised in that：The battery electrode paste include lithium ion battery just
Pole slurry or negative electrode slurry.
10. a kind of production method of lithium ion battery, it is characterised in that including：
Using point of detection method detection lithium ion battery anode glue size or negative electrode slurry described in any one of claim 1-9
Dissipate the uniformity；And
If it is determined that the dispersed homogeneous degree of the lithium ion battery anode glue size or negative electrode slurry is qualified, then lithium ion battery is being carried out just
The preparation of pole or cathode, conversely, then re-starting decentralized processing to the lithium ion battery anode glue size or negative electrode slurry.
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Application publication date: 20180717 |
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